CN106749967A - A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent - Google Patents
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent Download PDFInfo
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- CN106749967A CN106749967A CN201611089616.6A CN201611089616A CN106749967A CN 106749967 A CN106749967 A CN 106749967A CN 201611089616 A CN201611089616 A CN 201611089616A CN 106749967 A CN106749967 A CN 106749967A
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- vpeg
- organic solvent
- solid
- reducing agent
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2688—Copolymers containing at least three different monomers
- C04B24/2694—Copolymers containing at least three different monomers containing polyether side chains
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
Abstract
The invention discloses a kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprise the following steps：(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；(2) to the second mixed solution for the first mixed solution for being made up of acrylic acid, unsaturated phosphate monomer and unsaturated silane being added dropwise in the material obtained by step (1) respectively and be made up of initiator, chain-transferring agent and organic solvent, dripped off in 0.5~1h, continue anti-0.8~1.2h；(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, material is cut into slices by condensing slicer afterwards, obtains final product the solid collapse protective poly-carboxylic acid water reducing agent.Solid polycarboxylic acid water reducing agent prepared by the present invention has excellent diminishing dispersion effect, remains to show preferable mobility and holding capacity under compared with low-dosage, and cement to different cultivars shows very strong adaptability.
Description
Technical field
The invention belongs to build additive technical field, and in particular to a kind of preparation of solid collapse protective poly-carboxylic acid water reducing agent
Method.
Background technology
Polycarboxylate water-reducer sets as the BSA of modern concrete by its excellent low-dosage, high-thin arch dam, molecule
The advantages of meter free degree is big, is widely used in concrete works technical field.At present, wide variety of polycarboxylic acids diminishing
Agent is generally the solution product of 10-50% concentration.Transported into because part job location can improve apart from remote, relatively low solid content
This；In addition, the wide popularization and application of dry powder and mortar, also the production application of solid poly carboxylic acid series water reducer is proposed and compels to be essential
Ask.Powder poly carboxylic acid series water reducer in the market is generally to be obtained by spray drying process, but is diluted to liquid,
Performance has declined compared with the liquid poly carboxylic acid series water reducer with concentration, and this is mainly generation after poly carboxylic acid series water reducer is heated
It is partial cross-linked to cause.If expecting the poly carboxylic acid series water reducer powder product of excellent performance, can only be by the way of low temperature, no
Operated under conditions of destruction poly carboxylic acid series water reducer structure.
CN1919772A discloses a kind of preparation method of powder poly carboxylic acid series water reducer, is sprayed by by water reducer, heat
Air-dry dry realize.Production process high energy consumption, and poly carboxylic acid series water reducer can occur at high temperature it is partial cross-linked, control not
When, will a large amount of wall built-up, not only influence the quality but also wall built-up thing of powder product to be heated for a long time and be possible to trigger burning.
CN102372458A discloses a kind of preparation method of solid poly carboxylic acid series water reducer, by unsaturated acids with other not
Saturation monomer carries out copolymerization in organic organic solvent, is then prepared after separated precipitation and low temperature drying.The solid subtracts
In water organic solvent is dissolved in, compared with the liquid poly carboxylic acid series water reducer product of commercially available same concentration, combination property does not have aqua
It is variant.
At present, the preparation of solid polycarboxylic acid water reducing agent is preparation cost high, and instrument and equipment is expensive, and power consumption is high, while preparing
The polycarboxylate water-reducer for going out due to be not performance under 100% solid content and hot conditions loss, its water-reducing effect is subject to one
Determine the influence of degree.Therefore on the premise of polycarboxylate water-reducer performance is not lost, in the case of lower cost, eaily
Prepare the key that a kind of solid polycarboxylic acid water reducing agent is further genralrlization and application polycarboxylate water-reducer.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided a kind of preparation of solid collapse protective poly-carboxylic acid water reducing agent
Method.
Technical scheme is as follows：
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprises the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) to being added dropwise respectively by acrylic acid, unsaturated phosphate monomer and unsaturated silane in the material obtained by step (1)
First mixed solution of composition and the second mixed solution being made up of initiator, chain-transferring agent and organic solvent, in 0.5~1h
Inside drip off, continue anti-0.8~1.2h；
(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, the working machine pump time is 8
~12min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects
The type that collapses polycarboxylate water-reducer；
Wherein, above-mentioned unsaturated phosphate monomer is vinyl phosphonic diethyl phthalate or 2- methyl -2- acrylic acid phosphinylidynes
Three (epoxide -2,1- ethylidene) esters, above-mentioned unsaturated silane be γ-(methyl) acryloxypropyl trimethoxy silane or
γ-(methyl) acryloxypropyl triethoxysilane, above-mentioned VPEG monomers, acrylic acid, unsaturated phosphate monomer and not
The mol ratio of saturation silane is 1: 2.5: 0.5~1: 0.1-0.5.
In a preferred embodiment of the invention, the initiator is azo isobutyl cyano group formamide.
In a preferred embodiment of the invention, the chain-transferring agent is 3,6- dioxy -1, pungent two mercaptan of 8-.
In a preferred embodiment of the invention, the organic solvent is acetone, n-hexane or carbon tetrachloride.
It is further preferred that the consumption of the initiator is the 2~5% of VPEG monomer gross mass.
It is further preferred that the consumption of the chain-transferring agent is the 2~4% of VPEG monomer gross mass.
It is further preferred that the consumption of the organic solvent is the 20~50% of VPEG monomer gross mass.
Beneficial effects of the present invention：
1st, the weight average molecular weight of solid collapse protective poly-carboxylic acid water reducing agent prepared by the present invention is 30000~80000, with excellent
Different diminishing dispersion effect, remains to show preferable mobility and holding capacity under compared with low-dosage, and to different cultivars
Cement show very strong adaptability.Additionally, water reducer Product Status stabilization, deposits under low temperature and does not crystallize, and low-temperature storage
Performance is unaffected afterwards.
2nd, process is simple of the invention, controllability is strong, low cost, it is easy to industrialized production.
Specific embodiment
Technical scheme is further detailed and described below by way of specific embodiment.
Embodiment 1
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprises the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) to being added dropwise respectively by acrylic acid, vinyl phosphonic diethyl phthalate and γ-(methyl) in the material obtained by step (1)
Acryloxypropyl trimethoxy silane composition the first mixed solution and by azo isobutyl cyano group formamide, 3,6- bis-
Oxygen -1, pungent two mercaptan of 8-, the second mixed solution of acetone composition, drips off in 0.5~1h, continues anti-1h；
(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, the working machine pump time is
10min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects and collapses
Type polycarboxylate water-reducer, is packed finally by packing machine.Wherein：VPEG monomers, acrylic acid, unsaturated phosphate monomer and
The mol ratio of unsaturated silane is 1: 2.5: 0.5: 0.5, and it is mono- that the consumption of initiator, chain-transferring agent and organic solvent is respectively VPEG
5%, 3% and the 30% of body gross mass.
Embodiment 2
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprises the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) to being added dropwise respectively in the material obtained by step (1) by the acrylic acid, (oxygen of 2- methyl -2- acrylic acid phosphinylidyne three
Base -2,1- ethylidene) ester and γ-(methyl) acryloxypropyl triethoxysilane composition the first mixed solution and by
Azo isobutyl cyano group formamide, 3,6- dioxy -1, pungent two mercaptan of 8-, the second mixed solution of n-hexane composition, in 0.5~1h
Drip off, continue anti-1h；
(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, the working machine pump time is
10min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects and collapses
Type polycarboxylate water-reducer, is packed finally by packing machine.Wherein：VPEG monomers, acrylic acid, unsaturated phosphate monomer and
The mol ratio of unsaturated silane is 1: 2.5: 0.75: 0.25, and the consumption of initiator, chain-transferring agent and organic solvent is respectively VPEG
3%, 2% and the 50% of monomer gross mass.
Embodiment 3
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprises the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) to being added dropwise respectively by acrylic acid, vinyl phosphonic diethyl phthalate and γ-(methyl) in the material obtained by step (1)
Acryloxypropyl triethoxysilane composition the first mixed solution and by azo isobutyl cyano group formamide, 3,6- bis-
Oxygen -1, pungent two mercaptan of 8-, the second mixed solution of carbon tetrachloride composition, drips off in 0.5~1h, continues anti-1h；
(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, the working machine pump time is
10min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects and collapses
Type polycarboxylate water-reducer, is packed finally by packing machine.Wherein：VPEG monomers, acrylic acid, unsaturated phosphate monomer and
The mol ratio of unsaturated silane is 1: 2.5: 1: 0.1, and the consumption of initiator, chain-transferring agent and organic solvent is respectively VPEG monomers
2%, 4% and the 20% of gross mass.
Embodiment 4
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprises the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) to being added dropwise respectively in the material obtained by step (1) by the acrylic acid, (oxygen of 2- methyl -2- acrylic acid phosphinylidyne three
Base -2,1- ethylidene) ester and γ-(methyl) acryloxypropyl trimethoxy silane composition the first mixed solution and by
Azo isobutyl cyano group formamide, 3,6- dioxy -1, pungent two mercaptan of 8-, the second mixed solution of n-hexane composition, in 0.5~1h
Drip off, continue anti-1h；
(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, the working machine pump time is
10min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects and collapses
Type polycarboxylate water-reducer, is packed finally by packing machine.In：VPEG monomers, acrylic acid, unsaturated phosphate monomer and not
The mol ratio of saturation silane is 1: 2.5: 0.6: 0.4, and the consumption of initiator, chain-transferring agent and organic solvent is respectively VPEG monomers
4%, 2.5% and the 40% of gross mass.
Embodiment 1 to 4 is synthesized the sample for obtaining, using standard cement, volume presses cement quality 0.2%, according to GB
8076-2008《Concrete admixture》, survey its concrete water-reducing ratio, the slump and Slump Time losing of Large.Concrete mix
For：Cement 360kg/m3, sand 803kg/m3, stone 982kg/m3, the slump control in 210 ± 10mm, the acquired results such as institute of table 1
Show.
The concrete performance of the sample that table 1 is synthesized using embodiment
| Sample | Benchmark | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 |
| Water consumption/kg | 4020 | 2495 | 2573 | 2412 | 2533 |
| Water-reducing rate/% | / | 38 | 36 | 40 | 37 |
| Slump T0 | 205 | 215 | 220 | 210 | 210 |
| Through when slump T1h | 145 | 205 | 210 | 205 | 210 |
As shown in Table 1, using the present invention prepare solid collapse protective poly-carboxylic acid water reducing agent, with low-dosage, high water reducing rate,
Low slump loss and the good performance of adaptability.
Those of ordinary skill in the art understand, when technical scheme changes in following ranges, remain able to
To technical scheme same as the previously described embodiments or close, protection scope of the present invention is still fallen within：
A kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, comprises the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) to being added dropwise respectively by acrylic acid, unsaturated phosphate monomer and unsaturated silane in the material obtained by step (1)
First mixed solution of composition and the second mixed solution being made up of initiator, chain-transferring agent and organic solvent, in 0.5~1h
Inside drip off, continue anti-0.8~1.2h；
(3) organic solvent in removal step (2) resulting material is vacuumized using mechanical pump, the working machine pump time is 8
~12min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects
The type that collapses polycarboxylate water-reducer；
Wherein, above-mentioned unsaturated phosphate monomer is vinyl phosphonic diethyl phthalate or 2- methyl -2- acrylic acid phosphinylidynes
Three (epoxide -2,1- ethylidene) esters, above-mentioned unsaturated silane be γ-(methyl) acryloxypropyl trimethoxy silane or
γ-(methyl) acryloxypropyl triethoxysilane, above-mentioned VPEG monomers, acrylic acid, unsaturated phosphate monomer and not
The mol ratio of saturation silane is 1: 2.5: 0.5~1: 0.1-0.5, and the consumption of initiator, chain-transferring agent and organic solvent is respectively
2~5%, 2~4% and the 20~50% of VPEG monomer gross mass.
The above, is only presently preferred embodiments of the present invention, and not technical scope of the invention is imposed any restrictions,
Therefore the change or modification that claim under this invention and specification are done in every case, should all belong to the scope that patent of the present invention covers
Within.
Claims (7)
1. a kind of preparation method of solid collapse protective poly-carboxylic acid water reducing agent, it is characterised in that：Comprise the following steps：
(1) VPEG monomers are added in reactor, are warming up to 20~30 DEG C, be at molten condition；
(2) it is made up of acrylic acid, unsaturated phosphate monomer and unsaturated silane to being added dropwise respectively in the material obtained by step (1)
The first mixed solution and the second mixed solution for being made up of initiator, chain-transferring agent and organic solvent, dripped in 0.5~1h
It is complete, continue anti-0.8~1.2h；
(3) organic solvent in removal step (2) resulting material being vacuumized using mechanical pump, the working machine pump time is 8~
12min, vacuum pressure is 0.01-0.05MPa, and material is cut into slices by condensing slicer afterwards, obtains final product the solid and protects and collapses
Type polycarboxylate water-reducer；
Wherein, above-mentioned unsaturated phosphate monomer is vinyl phosphonic diethyl phthalate or the (oxygen of 2- methyl -2- acrylic acid phosphinylidyne three
Base -2,1- ethylidene) ester, above-mentioned unsaturated silane is γ-(methyl) acryloxypropyl trimethoxy silane or γ-(first
Base) acryloxypropyl triethoxysilane, above-mentioned VPEG monomers, acrylic acid, unsaturated phosphate monomer and unsaturated silicon
The mol ratio of alkane is 1: 2.5: 0.5~1: 0.1-0.5.
2. preparation method as claimed in claim 1, it is characterised in that：The initiator is azo isobutyl cyano group formamide.
3. preparation method as claimed in claim 1, it is characterised in that：The chain-transferring agent is 3,6- dioxy -1, pungent two sulphur of 8-
Alcohol.
4. preparation method as claimed in claim 1, it is characterised in that：The organic solvent is acetone, n-hexane or four chlorinations
Carbon.
5. the preparation method as described in any claim in Claims 1-4, it is characterised in that：The consumption of the initiator
It is the 2~5% of VPEG monomer gross mass.
6. the preparation method as described in any claim in Claims 1-4, it is characterised in that：The use of the chain-transferring agent
Measure is the 2~4% of VPEG monomer gross mass.
7. the preparation method as described in any claim in Claims 1-4, it is characterised in that：The use of the organic solvent
Measure is the 20~50% of VPEG monomer gross mass.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107629163A (en) * | 2017-10-09 | 2018-01-26 | 常州凯恒纺织品有限公司 | A kind of preparation method of polycarboxylate water-reducer |
| CN108003304A (en) * | 2017-12-28 | 2018-05-08 | 科之杰新材料集团有限公司 | A kind of preparation method of modified by cardanol esters polycarboxylate water-reducer |
| CN111825373A (en) * | 2020-08-11 | 2020-10-27 | 贵州石博士科技有限公司 | Preparation method for synthesizing high-performance polycarboxylate superplasticizer from novel VPEG polyether |
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| CN103073687A (en) * | 2013-01-18 | 2013-05-01 | 科之杰新材料集团有限公司 | Method for preparing high-dispersity polycarboxylic super plasticizer |
| CN103848944A (en) * | 2013-05-14 | 2014-06-11 | 科之杰新材料集团有限公司 | Preparation method of super-retarding type polycarboxylate superplasticizer |
| CN106046269A (en) * | 2016-06-22 | 2016-10-26 | 科之杰新材料集团有限公司 | Crosslinking-type low-sensitivity ester-ether copolymerized polycarboxylate superplasticizer and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103073687A (en) * | 2013-01-18 | 2013-05-01 | 科之杰新材料集团有限公司 | Method for preparing high-dispersity polycarboxylic super plasticizer |
| CN103848944A (en) * | 2013-05-14 | 2014-06-11 | 科之杰新材料集团有限公司 | Preparation method of super-retarding type polycarboxylate superplasticizer |
| CN106046269A (en) * | 2016-06-22 | 2016-10-26 | 科之杰新材料集团有限公司 | Crosslinking-type low-sensitivity ester-ether copolymerized polycarboxylate superplasticizer and preparation method thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107629163A (en) * | 2017-10-09 | 2018-01-26 | 常州凯恒纺织品有限公司 | A kind of preparation method of polycarboxylate water-reducer |
| CN108003304A (en) * | 2017-12-28 | 2018-05-08 | 科之杰新材料集团有限公司 | A kind of preparation method of modified by cardanol esters polycarboxylate water-reducer |
| CN111825373A (en) * | 2020-08-11 | 2020-10-27 | 贵州石博士科技有限公司 | Preparation method for synthesizing high-performance polycarboxylate superplasticizer from novel VPEG polyether |
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